%0 Journal Article %A Donzello, Maria Pia %A Ercolani, Claudio %A Chiesi-Villa, Angiola %A Rizzoli, Corrado %D 1998 %T One Step Forward to “Stapled” Bis(phthalocyanine) Metal Complexes:  Synthesis, Characterization, and Redox Properties of Bis(phthalocyaninato)niobium(IV). X-ray Crystal Structure of the Monoelectronically Oxidized Species [Pc2Nb](I3)(I2)0.5(ClNP)3.5 (ClNP = 1-Chloronaphthalene) %U https://acs.figshare.com/articles/journal_contribution/One_Step_Forward_to_Stapled_Bis_phthalocyanine_Metal_Complexes_Synthesis_Characterization_and_Redox_Properties_of_Bis_phthalocyaninato_niobium_IV_X-ray_Crystal_Structure_of_the_Monoelectronically_Oxidized_Species_Pc_sub_2_sub_Nb_I_sub_3_sub_I_sub_2_sub_su/3619851 %R 10.1021/ic970841f.s002 %2 https://acs.figshare.com/ndownloader/files/5708478 %K Pc 2 Nb %K C 11A %K Step Forward %K saltlike species %K UV %K C 31A %K Redox Properties %K Monoelectronically Oxidized Species %K ClNP %X Bis(phthalocyaninato)niobium(IV) has been prepared and isolated as a monosolvate, [Pc2Nb]·ClNP (ClNP = 1-chloronaphthalene). It is a light-brown, stable-to-air Nb(IV) (d1) paramagnetic sandwich-like species, which, upon oxidation by I2 under mild conditions, undergoes a metal-centered monoelectronic oxidation to give the diamagnetic Nb(V) (d0) [Pc2Nb]+ fragment, with formation of saltlike species of formula [Pc2Nb](I3)(I2)0.5(ClNP)3.5 (I). The structure of I has been elucidated by single-crystal X-ray work. Crystals are triclinic:  formula C64H32N16Nb·I3·0.5I2·3.5C10H7Cl, M = 2194.8, a = 17.702(3) Å, b = 18.708(3) Å, c = 13.504(2) Å, V = 4267.5(13) Å3, α = 106.00(2)°, β = 93.39(2)°, γ = 83.26(1)°, Z = 2, space group P1̄. The structure of the [Pc2Nb]+ fragment, “stapled” by two inter-ligand C−C σ bonds (C11A−C11B and C31A−C31B = 1.574(15) Å), together with its color and UV−visible spectral behavior, allows a straightforward assignment of the same “stapled” structure to the unoxidized [Pc2Nb]. The present niobium sandwiched materials reiterate the peculiar structural findings shown only by the previously reported [Pc2Ti]. %I ACS Publications